Amino Fonksiyonlu TiO2 Nanoparçacıkları Kullanılarak Diş Kompozitlerinin Geliştirilmesi ve Karakterizasyon

Öz

Amaç: Titanyum dioksit, benzersiz fizikokimyasal özellikleri nedeniyle çeşitli endüstriyel uygulamalarda yaygın olarak kullanılmaktadır. Bu çalışma, fonksiyonelleştirilmiş titanyum dioksit (TiO2-NH2) ve silika nanopartiküllerin (SiO2), diş dolgu malzemeleri kullanılarak tasarlanan diş kompozitlerinin fizikokimyasal özellikleri ve antibakteriyel aktiviteleri üzerindeki etkilerini araştırmayı amaçlamaktadır. Yöntem: Fonksiyonel titanyum bileşikleri içeren diş kompozitinin sentezi, Fourier Dönüşümlü Kızılötesi Spektroskopisi (FTIR) kullanılarak ve yüzey morfolojisi Taramalı Elektron Mikroskobu (SEM) kullanılarak doğrulanmıştır. Diş kompozitlerinin termal kararlılığı Termal Gravimetrik Analiz (TGA) ile kanıtlanmıştır. Diş kompozitlerinin su emilimi, suda çözünürlüğü ve kimyasal kararlılığı incelenmiştir. Minimum İnhibitör Konsantrasyon (MİK) ve Minimum Bakterisidal Konsantrasyon (MBK) testleri kullanılarak Escherichia coli (E. coli) ve Staphylococcus aureus (S. aureus) bakterilerine karşı antibakteriyel aktivite belirlenmiştir. Bulgular: Su emilimi ve suda çözünürlüğünün ISO standartlarına uygun olduğu gözlemlenmiştir. Fenton testi sonuçları, dental kompozitlerin kimyasal olarak kararlı olduğunu ve maksimum malzeme kaybının yaklaşık %0,19 olduğunu göstermiştir. Titanyum nanopartiküllerin yüzey fonksiyonelleştirilmesi antibakteriyel aktiviteyi artırmış ve nanopartiküllerin gram negatif bakteri türü E. coli'ye karşı daha etkili olduğu gözlemlenmiştir. Sonuç: Dental kompozitlere fonksiyonel titanyum nanopartiküllerin dahil edilmesi, fizikokimyasal ve antibakteriyel özelliklerinde önemli gelişmeler sağlamıştır. Bulgular, sentezlenen bu kompozitlerin çeşitli endüstriyel uygulamalarda kullanılma potansiyelini desteklemektedir.

Anahtar Kelimeler

• Antibakteriyel aktivite
• Dental kompozit
• Silika
• Titanyum dioksit

DEVELOPMENT AND CHARACTERIZATION OF DENTAL COMPOSITES USING AMINO-FUNCTIONALIZED TIO2 NANOPARTICLES

Öz

Objective: Titanium dioxide (TiO2) is extensively utilized in various industrial applications owing to its unique physicochemical properties. This study aimed to evaluate the effects of amino-functionalized titanium dioxide nanoparticles (TiO2-NH2) and silica nanoparticles (SiO2) on the development and characterization of dental composites formulated using conventional dental restorative materials. Method: The successful synthesis of the dental composite series incorporating functional titanium compounds was confirmed via Fourier Transform Infrared Spectroscopy (FTIR). The surface morphology was analyzed using Scanning Electron Microscopy (SEM). Furthermore, the thermal stability of dental composites was assessed by Thermogravimetric Analysis (TGA). The water sorption, water solubility, and chemical stability of the composites were meticulously investigated. Antibacterial activity of TiO2, and TiO2-NH2 nanoparticles were determined against the Gram-negative strain Escherichia coli (E. coli) and the Gram-positive strain Staphylococcus aureus (S. aureus) using Minimum Inhibitory Concentration (MIC) and Minimum Bactericidal Concentration (MBC) assays. Results: The evaluation of water sorption and water solubility confirmed that the dental composites conformed to the established ISO standards. Furthermore, Fenton testing results demonstrated the chemical stability of the composites, revealing a negligible maximum material loss of approximately 0.19%. Notably, the surface functionalization of the titanium nanoparticles significantly enhanced their antibacterial efficacy. This enhanced activity was predominantly observed against the Gram-negative bacterial species, E. coli. Conclusion: The successful incorporation of amino-functionalized titanium nanoparticles into the dental composite matrix led to significant enhancements in both their physicochemical and antibacterial properties. Overall, these robust findings strongly affirm the potential of the synthesized dental composites for deployment in a broad spectrum of biomedical and industrial applications.

Anahtar Kelimeler

• Antibacterial activity
• Dental composite
• Silica
• Titanium dioxide

Kaynakça

1. Yang DL, Cui YN, Sun Q, Liu M, Niu H, Wang JX. Antibacterial activity and reinforcing effect of SiO2-ZnO complex cluster fillers for dental resin composites. Biomaterials Science. 2021;9(5): 1795–1804. doi:10.1039/D0BM01834A
2. Garibay-Alvarado JA, Garcia-Zamarron DJ, Silva-Holguín PN, Donohue-Cornejo A, Cuevas-González JC, Espinosa-Cristóbal LF, Ruíz-Baltazar ÁJ, Reyes-López SY. Polymer-Based Hydroxyapatite–Silver Composite Resin with Enhanced Antibacterial Activity for Dental Applications. Polymers. 2024;16(14). doi:10.3390/polym16142017
3. Lee H, Kim YJ, Yang YJ, Lee JH, Lee HH. Development of antibacterial dual-cure dental resin composites via tetrapod-shaped zinc oxide incorporation. Dental Materials. 2024. doi: 10.1016/j.dental.2024.07.021
4. Elfakhri F, Alkahtani R, Li C, Khaliq J. Influence of filler characteristics on the performance of dental composites: A comprehensive review. In Ceramics International. 48th ed. Elsevier Ltd.; 2022: 27280–27294. doi: 10.1016/j.ceramint.2022.06.314
5. Jenima J, Priya Dharshini M, Ajin ML, Jebeen Moses J, Retnam KP, Arunachalam KP, Avudaiappan S, Arrue Munoz RF. A comprehensive review of titanium dioxide nanoparticles in cementitious composites. Heliyon. 2024; 10:20. doi: 10.1016/j.heliyon. 2024.e39238
6. Chandrasekaran R. Harnessing the functional role of polymeric nanocomposite in dental caries disease: A comprehensive review. In Hybrid Advances. 10th ed. Elsevier B.V.; 2025. doi: 10.1016/j.hybadv.2025.100433
7. Bhadila GY, Baras BH, Balhaddad AA, Williams MA, Oates TW, Weir M D, Xu HHK. Recurrent caries models to assess dental restorations: A scoping review. In Journal of Dent. 136th ed. Elsevier Ltd.; 2023. doi: 10.1016/j.jdent.2023.104604
8. Pourhajibagher M, Bahrami R, Bahador A. Application of photosensitive dental materials as a novel antimicrobial option in dentistry: A literature review. In Journal of Dental Sciences. 2024;19(2):762-772. doi: 10.1016/j.jds.2023.12.019

9. Kaptan Usul S, Aslan A, Lüleci HB, Ergüden B. Effects of Hexagonal Boron Nitride and Mesoporous Silica Nanoparticles on the Morphology, Mechanical Properties and Antimicrobial Activity of Dental Composites. Journal of Cluster Science. 2024;35(7):2293–2309. doi:10.1007/s10876-024-02658-1
10. Cho K, Rajan G, Farrar P, Prentice L, Prusty BG. Dental resin composites: A review on materials to product realizations. In Composites Part B: Engineering. 230 th ed. Elsevier Ltd.; 2022. doi: 10.1016/j.compositesb.2021.109495 11. Melo MAS, Mokeem L, Sun J. Bioactive Restorative Dental Materials—The New Frontier. In Dental Clinics of North America. 2022;66(4):551–566. doi: 10.1016/j.cden.2022.05.005
11. Li B, Wu J, Dong Y, Qiu D. Bioactive glass empowered growable composite resin enabling a seamless dental caries filling. Composites Part A: Applied Science and Manufacturing. 2025;189. doi: 10.1016/j.compositesa.2024.108621
12. Saini S, Meena A, Yadav R, Patnaik A. Fabrication, Evaluation, and Performance Ranking of Tri-calcium Phosphate and Silica Reinforced Dental Resin Composite Materials. Silicon. 2013;15(18):8045–8063. doi:10.1007/s12633-023-02646-6
13. Buchwald Z, Sandomierski M, Smułek W, Ratajczak M, Patalas A, Kaczorek E, Voelkel A. Physical–chemical and biological properties of novel resin-based composites for dental applications. Polymer Bul. 2023;80(10):11249–11272. doi:10.1007/s00289-022-04606-3
14. Zinina EM, Savinkov VI, Klimenko NN, Ivanova ED, Brusentseva AL, Buzov AA, Chuev VP, Sigaev VN. SrO–Al2O3–B2O3–SiO2-Based Glass Fillers for Dental Filling Composites. Glass and Ceramics. 2023;79(11–12):491–496. doi:10.1007/s10717-023-00538-0
15. Garcia IM, Souza VS, Balhaddad AA, Mokeem L, Melo MAS, Scholten JD, Collares FM. Ionic Liquid-Based Silane for SiO2 Nanoparticles: A Versatile Coupling Agent for Dental Resins. ACS Applied Materials and Interfaces. 2024;16(26):34057–34068. doi:10.1021/acsami.4c04580
16. Pavanello L, Cortês IT, Carvalho RDP, Picolo MZD, Cavalli V, Silva LTS, Boaro LCC, Prokopovich P, Cogo-Müller K. Physicochemical and biological properties of dental materials and formulations with silica nanoparticles: A narrative review. In Dental Materials. 2024. doi: 10.1016/j.dental.2024.07.028
17. Wang Y, Zhang H, Li H, Yao X, Hang R. Zr-doped mesoporous silica (Zr-MSS) for improved mechanical stability and biocompatibility of dental composite resins. Journal of the Mechanical Behavior of Biomedical Materials. 2025;164. doi: 10.1016/j.jmbbm.2025.106902
18. Sharma H, Pathak M. Development of PCL/TiO2 composite as an efficient antibacterial, anticancer drug and biocompatible properties. Results in Chemistry. 2024;7. doi: 10.1016/j.rechem.2024.101534
19. Zhou S, Deng C, Liu H, Sun Y, Zhang J. Investigating the antibacterial activity of Thyme Oil/TiO2 modified resins against oral pathogenic bacteria. Alexandria Engineering Journal. 2024;89: 195–201. doi: 10.1016/j.aej.2024.01.041
20. Ahmad Fauzi NA, Ireland AJ, Sherriff M, Bandara HMHN, Su B. Nitrogen doped titanium dioxide as an aesthetic antimicrobial filler in dental polymers. Dental Materials. 2022;38(1):147–157. doi: 10.1016/j.dental.2021.10.019
21. Ravandi R, Zeinali Heris S, Hemmati S, Aghazadeh M, Davaran S, Abdyazdani N. Effects of chitosan and TiO2 nanoparticles on the antibacterial property and ability to self-healing of cracks and retrieve mechanical characteristics of dental composites. Heliyon. 2024;10(6). doi: 10.1016/j.heliyon. 2024.e27734
22. Guimarães GMF, Bronze-Uhle ES, Lisboa-Filho PN, Fugolin APP, Borges AFS, Gonzaga CC, Pfeifer CS, Furuse AY. Effect of the addition of functionalized TiO2 nanotubes and nanoparticles on properties of experimental resin composites. Dental Materials. 2020;36(12):1544–1556. doi: 10.1016/j.dental.2020.09.013
23. Dafar MO, Grol MW, Canham PB, Dixon SJ, Rizkalla AS. Reinforcement of flowable dental composites with titanium dioxide nanotubes. Dental Materials. 2016; 32(6):817–826. doi: 10.1016/j.dental.2016.03.022
24. Yadav R, Meena A. Effect of aluminium oxide, titanium oxide, hydroxyapatite filled dental restorative composite materials on physico-mechanical properties. Ceramics International. 2022;48(14):20306–20314. doi:10.5281/ZENODO.16959306
25. Sienkiewicz A, Wanag A, Kusiak-Nejman E, Ekiert E, Rokicka-Konieczna P, Morawski AW. Effect of calcination on the photocatalytic activity and stability of TiO2 photocatalysts modified with APTES. Journal of Environmental Chemical Engineering. 2021;9(1). doi: 10.1016/j.jece.2020.104794
26. Aslan A, Kaptan Usul S. Dental uygulamalar için yeni nesil fonksiyonel nanokompozitlerin hazırlanması ve karakterizasyonu. İnönü Üniversitesi Sağlık Hizmetleri Meslek Yüksek Okulu Dergisi. 2021;9(3):1027–1043. doi:10.33715/inonusaglik.850453
27. Sousa MGC, Xavier PD, Cantuária APDC, Porcino RA, Almeida JA, Franco OL, Rezende TMB. Host defense peptide IDR-1002 associated with ciprofloxacin as a new antimicrobial and immunomodulatory strategy for dental pulp revascularization therapy. Microbial pathogenesis. 2021; 152:104634. doi: 10.1016/j.micpath.2020.104634
28. Xie SX, Song L, Yuca E, Boone K, Sarikaya R, VanOosten SK, Tamerler C. Antimicrobial peptide–polymer conjugates for dentistry. ACS applied polymer materials. 2020;2(3):1134-1144. doi:10.1021/acsapm.9b00921
29. Kaptan Usul S, Aslan A, Lüleci HB, Ergüden B, Çöpoğlu MT, Oflaz H, Soydan AM, Özçimen D. Investigation of antimicrobial and mechanical effects of functional nanoparticles in novel dental resin composites. Journal of Dentistry. 2022;123. doi: 10.1016/j.jdent.2022.104180
30. Dalod ARM, Grendal OG, Skjærvø SL, Inzani K, Selbach SM, Henriksen L, Van Beek W, Grande T, Einarsrud MA. Controlling Oriented Attachment and in Situ Functionalization of TiO2 Nanoparticles during Hydrothermal Synthesis with APTES. Journal of Physical Chemistry C. 2017;121(21):11897–11906. doi: 10.1021/acs.jpcc.7b02604
31. Vatansever F, Melo WCMA, Avci P, Vecchio D, Sadasivam M, Gupta A, Chandran R, Karimi M, Parizotto NA, Yin R, Tegos GP, Hamblin MR. Antimicrobial strategies centered around reactive oxygen species-bactericidal antibiotics, photodynamic therapy, and beyond. In FEMS Microbiology Reviews. 2013;37(6):955–989. doi:10.1111/1574-6976.12026
32. Chaughule R, Raorane D, Pednekar S, Dashaputra R. Nanocomposites and their use in dentistry. In Dental Applications of Nanotechnology. Springer International Publishing; 2018. doi:10.1007/978-3-319-97634-1_4
33. Fernández-Garrido P, Fernández-Dominguez P, Fernández De La Fuente L, Manso De Gustin B, Varona JF, Bosch BM, Fernández-Domínguez M. Citric acid-based solutions as decontaminant mouthwash in titanium and dental prostheses materials in implantoplasty processes. Prosthesis. 2024;6(5):1211-1227. doi.org/10.3390/prosthesis6050087
34. Cherchali FZ, Attik N, Issaadi HM, Abouelleil H, Decoret D, Amirouche-Korichi A, Grosgogeat B. Integration of various forms of Salvadora Persica «Siwak» into dental composites: A pilot in vitro study. Dental Materials. 2025;1120-1130. doi.org/10.1016/j.dental.2025.06.015